CN104231751B - A kind of electroconductive printing ink preparation method for gas sensor electrode material - Google Patents
A kind of electroconductive printing ink preparation method for gas sensor electrode material Download PDFInfo
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- CN104231751B CN104231751B CN201410442570.6A CN201410442570A CN104231751B CN 104231751 B CN104231751 B CN 104231751B CN 201410442570 A CN201410442570 A CN 201410442570A CN 104231751 B CN104231751 B CN 104231751B
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Abstract
The invention belongs to printed electronics field, be specifically related to a kind of electroconductive printing ink preparation method for gas sensor electrode material.It concretely comprises the following steps: mixed with superconduction carbon black by modified urea-formaldehyde resin, and adding weight fraction is the firming agent of 5 wt% and appropriate reactive diluent, can be prepared by the electroconductive printing ink for sensor electrode material.Obtaining printed pattern through heat cure, its resistivity more than 250 DEG C, passes through scanning electron microscopic observation at 1 ~ 5 Ω m, heat decomposition temperature, it can be seen that the carbon powder particle after solidification presents the network structure of densification.The electrically conductive ink using this method to prepare, has viscosity easy to control, it is adaptable to all kinds of printing technologies, includes but not limited to the emerging addition process technique such as inkjet printing, aerosol injection printing, be also applicable to traditional handicraft such as silk screen printing, intaglio printing etc..Compared to the method preparing chemical sensor electrode material at present, save cost greatly.
Description
Technical field
The invention belongs to printed electronics technical field of ink, relate to a kind of conduction for gas sensor electrode material
Printing-ink preparation method, it is adaptable to printed electronic prepares sensor electrode material, is particularly well-suited to emerging additive process such as
Aerosol injection printing, inkjet technology etc..
Background technology
Gas sensor is critically important a kind of sensor, and it is changed by gaseous species and with concentration dependent information
Become the signal of telecommunication, be obtained with the letter relevant with gas to be measured existence situation in the environment according to the power of these signals of telecommunication
Breath, such that it is able to carry out detecting, monitor, report to the police；Can also automatically detect by interface circuit with computer composition, control and report
Alarm system.Be now widely used for the detection of CO (carbon monoxide converter) gas, the detection of methane gas, the detection of coal gas, ammonia detection,
The detection of ethanol, the detection etc. of human oral cavity halitosis in the detection of freon (R11, R12), expiration.Setting at gas sensor
In meter, the selection of sensitive resistance is a key, because if sensitive resistance selects inappropriate, may cause the spirit of element
Sensitivity declines, and sensitive gas does not have susceptiveness the most to external world.
In view of the miniaturization of device and be easy to integrated, the employing that current gas sensor is relatively more has interdigital
The electrode of structure, fills sensitive material, as sensitive resistance between this electrode.Interdigital electrode is used in resistance type sensor
As signal electrode, its general shape is as it is shown in figure 1, major advantage is to reduce device size and easily controllable
The wherein size of sensitive resistance.The manufacture method of traditional interdigital electrode mainly uses magnetron sputtering method preparation gold interdigital electrode,
Firstly the need of customization mask blank, being cleaned by substrate, polished, acetone, dehydrated alcohol and deionized water process post-drying, adopt
With sol evenning machine, KW-4A type photoresist is uniformly coated on substrate, then mask plate as top and is put into photo-etching machine exposal and shown
Shadow, more above-mentioned substrate is put into magnetron sputter splash-proofing sputtering metal electrode, eventually pass ultrasonic stripping, and clean i.e. with acetone soln
Available interdigital electrode.
The method prepares interdigital electrode, although have preferably lifting in electrode precision, but owing to magnetron sputtering technique is formed
Metal layer thickness relatively thin, in order to meet sensor electrode requirement, often use gold or platinum as electrode material, technique is multiple
Miscellaneous and relatively costly.
The present invention uses the method for Lauxite mixing superconduction white carbon black to prepare conductive ink, owing to Lauxite itself has
The feature that cure shrinkage is big, even if using the carbon powder particle ink of relatively low-solid content, ink after overcuring due to bigger
Volume contraction so that carbon powder particle arrangement is more tight, is effectively increased electrical conductivity.Contrast through document, use ordinary resin
The conductive pattern resistivity that mixing superconduction carbon dust (carbon powder content is more than 20wt%) prepares is at 100 more than Ω m.And use
The present invention, uses 5wt% carbon dust mixing Lauxite, can yield less than the conductive pattern of 5 Ω m.Simultaneously as use print
Brush technology prepares electrode material, substantially reduces the preparation process of electrode material, compare employing magnetron sputtering method use gold, platinum be
Raw material, the ink with carbon dust as conductive filler has more advantage on cost, and meanwhile, the method that employing is repeatedly printed can be effective
Solve the problem that electrode layers thickness is relatively thin, effectively raise the electrical conductivity of electrode.
Summary of the invention
Present invention aim at providing a kind of electroconductive printing ink preparation method for gas sensor electrode material, should
It is easy to control that ink has viscosity, it is adaptable to all kinds of printing technologies, includes but not limited to that inkjet printing, aerosol injection printing etc. are new
Emerging addition process technique, is also applicable to traditional handicraft such as silk screen printing, intaglio printing etc..Compared to traditional preparation technology, stream
Journey significantly shortens, and cost is significantly reduced simultaneously.
The electroconductive printing ink preparation method for gas sensor electrode material that the present invention proposes, concrete steps are such as
Under:
By modified urea-formaldehyde resin, carbon dust mixes with firming agent, simultaneously according to printing ink printing art requirement, adds activity dilution
Agent regulation ink viscosity, can be prepared by the electroconductive printing ink for sensor electrode material, and wherein, the weight fraction of carbon dust is
3.5 ~ 25 wt%, the weight fraction of firming agent is 5 wt%, and the weight fraction of reactive diluent is 0-20wt%, and remaining is modified urea
Urea formaldehyde, its gross weight mark meets 100%.
In the present invention, described modified urea-formaldehyde resin is for using 1.5wt% polyvinyl alcohol (PVA) with 4wt% tripolycyanamide for changing
Property the modified Lauxite of agent, specifically comprise the following steps that
(1) PVA, PVA that add carbamide total amount 1.5% weight ratio use a small amount of boiling water pre-activate, and use 1% (with enforcement
In example, data are different) sodium hydroxide solution regulation pH=8 ~ 9, make the hydrogen bond formed between PVA construction unit be destroyed, improve it anti-
Should activity；
(2) being joined in there-necked flask with first carbamide by formaldehyde and react, controlling aldehyde urea is 2 than F/U, uses 1% hydrogen-oxygen
Change sodium solution to be regulated between 7 ~ 8 by pH value, react 5 ~ 8 min at (without this step in embodiment) 45 DEG C, be subsequently added step
(1) the preactivated PVA of gained, is gradually heating to 75 DEG C of reaction 30 min；Then it is cooled to 70 DEG C, adds second batch carbamide and make
F/U is 1.5, is 5 ~ 6 with 1% NaOH solution regulation system pH value；After stopping heating continuation reaction 30 minutes, use 1% sodium hydroxide
Solution regulation pH value is 7 ~ 8, and the tripolycyanamide adding the 3rd batch of carbamide and carbamide gross weight 4% makes F/U be 1.4, reacts 30 points
Clock, is cooled to less than 40 DEG C rapidly by system, and discharging obtains modified urea-formaldehyde resin.
In the present invention, the carbon dust used is superconduction white carbon black, and particle diameter is 10 ~ 20nm, and resistivity is 0.8-1.0 Ω m,
Content of ashes is less than 1.5%, does not allow containing semolina, and remaining index meets GB/T3782-2006 standard.
One or more in the present invention, in used firming agent aminoacid, organic dibasic acid or anhydride.
In the present invention, the reactive diluent used is the Lauxite of low-solid content, and its solidification amount is less than 20%, sticks
Degree is less than 20 mpa.s.
In the present invention, the preparation method of the Lauxite of described low-solid content is three feeding methods.By formaldehyde and first
Carbamide (F/U is 2) addition there-necked flask reacts, with 1% sodium hydroxide solution, pH value is regulated between 7 ~ 8, anti-at 45 DEG C
Answer 5 ~ 8 min, be gradually heating to 75 DEG C of reaction 30 min subsequently.It is cooled to 70 DEG C, adds second batch carbamide and make F/U1.5, use
10% ammonium chloride solution regulation system pH value is about 5 ~ 6.After stopping heating continuation reaction 30 minutes, use 1% sodium hydroxide solution
Regulation pH value, 7 ~ 8, adds the 3rd batch of carbamide and makes F/U be 1.4, react 30 minutes, rapidly system is cooled to less than 40 DEG C,
Discharging, obtains the Lauxite of low-solid content.
In the present invention, used typography viscosity requires and reactive diluent addition is as follows:
When printing process uses gas jet to print, controlling to rotate viscosity is 10 ~ 3000mpa.s, and reactive diluent adds
Amount is 5wt% ~ 20wt%, and carbon dust weight fraction is 3.5-15%；
When printing process uses inkjet printing, controlling to rotate viscosity is 10 ~ 80mpa.s, and reactive diluent addition is
15wt ~ 20wt%, carbon dust weight fraction is 3.5-10%；
When printing process uses silk screen printing, controlling to rotate viscosity is 10000 ~ 20000mpa.s, is added without activity dilution
Agent, carbon dust weight fraction is 20-25%；
When printing process uses intaglio printing, and control Engler degree is 15 ~ 26s, is added without reactive diluent, carbon dust weight
Mark is 15-25%.
In the present invention, it is easy to control that prepared ink has viscosity, it is adaptable to all kinds of printing technologies, includes but not limited to spray
Ink prints, aerosol injection prints, in silk screen printing or intaglio printing any one.
In the present invention, gained solidification its resistivity of figure is at 1 ~ 5 Ω m, and heat decomposition temperature is more than 250 DEG C, by scanning
Electron microscopic observation, it can be seen that the carbon powder particle after solidification presents the network structure of densification.
In the present invention, the curing of used ink is 60 DEG C of pre-solid 10min, 120 DEG C of solidification 15min.
According to the ink prepared by the present invention, there is viscosity easy to control, it is adaptable to all kinds of printing technologies, include but not limited to
The emerging addition process techniques such as inkjet printing, aerosol injection printing, are also applicable to traditional handicraft such as silk screen printing, intaglio printing
Deng.
According to the present invention, gained solidification its resistivity of figure is at 1 ~ 5 Ω m, and heat decomposition temperature is more than 250 DEG C, by sweeping
Retouch electron microscopic observation, it can be seen that the carbon powder particle after solidification presents the network structure of densification.
Currently as gas sensor electrode material ink, domestic having no is reported and is sold, and the present invention has:
1, reactions steps is simple, and mild condition, reaction raw materials is cheap and easy to get.
2, product cost is low, and processing technology is simple.
Accompanying drawing explanation
Fig. 1 is interdigitated electrode structure schematic diagram.
Fig. 2 is that embodiment 2 aerosol injection prints interdigital electrode sample.(a) be pet substrate print 1 this, (b) is PET
Substrate prints 5 times, and (c) is that PI substrate prints once, and (d) is that PI substrate prints 5 times
Fig. 3 embodiment 2 figure (b) pet substrate prints the scanning electron microscope (SEM) photograph (380x) of 5 times.
Detailed description of the invention
The following examples are to further illustrate the present invention rather than limit the scope of the present invention.
Embodiment 1:
Take 2.4g PVA be dissolved in 5ml boiling water activation be placed in 1L three-necked bottle, with 0.1% NaOH solution regulate pH to 8 ~ 9.
110g formaldehyde and 110g carbamide being mixed and add three-necked bottle, 45 DEG C of reactions 5-8min, about 30min are warming up to 75 DEG C, constant temperature
30min, regulates pH value between 7 ~ 8 with 1% sodium hydroxide solution.Add carbamide 37g, be cooled to 70 DEG C, use 1% NaOH
Solution regulation pH to 5 ~ 6.Stop heating after reaction 30min, be incubated 30min.Continuously add carbamide 10g and tripolycyanamide 6.3g,
And regulate pH to 7 ~ 8 by 1% NaOH solution.Reaction 30min, is cooled to less than 40 DEG C rapidly by system, and discharging obtains modified urea
Urea formaldehyde.
Taking 110g formaldehyde and the mixing of 110g carbamide adds in three-necked bottle, 45 DEG C of reactions 5-8min, about 30min are warming up to 75
DEG C, constant temperature 30min.Add carbamide 37g, be cooled to 70 DEG C, with 10% ammonium chloride solution regulation pH to 5 ~ 6.After reaction 30min
Stop heating, be incubated 30min.Continuously add carbamide 10g, and regulate pH to 7 ~ 8 by 1% NaOH solution.Reaction 30min, rapidly
System is cooled to less than 40 DEG C, and discharging obtains low-solid content Lauxite.
Take modified urea-formaldehyde resin 65 parts, superconduction white carbon black 15 parts, low-solid content Lauxite 15 parts, firming agent glycine 5 parts.
Electrically conductive ink is obtained with three-roller mix homogeneously., viscosity is 20000mpa.s, uses silk screen printing to prepare interdigital electrode,
60 DEG C of solidification 10min, solidify 15min in being placed in 120 DEG C of vacuum drying ovens and obtain electrode.Through test, its resistivity after solidification
Being 1.8 Ω m, heat decomposition temperature is 260 DEG C.
Embodiment 2
Take 2.4g PVA be dissolved in 5ml boiling water activation be placed in 1L three-necked bottle, with 0.1% NaOH solution regulate pH to 8 ~ 9.
110g formaldehyde and 110g carbamide being mixed and add three-necked bottle, 45 DEG C of reactions 5-8min, about 30min are warming up to 75 DEG C, use 1% hydrogen-oxygen
Change sodium solution to be regulated between 7 ~ 8 by pH value, constant temperature 30min.Add carbamide 37g, be cooled to 70 DEG C, use 1% NaOH solution
Regulation pH to 5 ~ 6.Stop heating after reaction 30min, be incubated 30min.Continuously add carbamide 10g and tripolycyanamide 6.3g, and use
1% NaOH solution regulation pH to 7 ~ 8.Reaction 30min, is cooled to less than 40 DEG C rapidly by system, and discharging obtains modified urea-formaldehyde tree
Fat.
Taking 110g formaldehyde and the mixing of 110g carbamide adds in three-necked bottle, 45 DEG C of reactions 5-8min, about 30min are warming up to 75
DEG C, constant temperature 30min.Add carbamide 37g, be cooled to 70 DEG C, with 10% ammonium chloride solution regulation pH to 5 ~ 6.After reaction 30min
Stop heating, be incubated 30min.Continuously add carbamide 10g, and regulate pH to 7 ~ 8 by 1% NaOH solution.Reaction 30min, rapidly
System is cooled to less than 40 DEG C, and discharging obtains low-solid content Lauxite.
Take modified urea-formaldehyde resin 65 parts, superconduction white carbon black 10 parts, low-solid content Lauxite 20 parts, firming agent phthalic acid
Acid anhydride 5 parts.Electrically conductive ink is obtained with three-roller mix homogeneously.Viscosity is 600mpa.s, uses aerosol injection to print and prepares
Interdigital electrode, 60 DEG C of solidification 10min, in being placed in 120 DEG C of vacuum drying ovens, solidify 15min obtain electrode, as shown in Figure 2.Pass through
Test, after solidification, its resistivity is 4.1 Ω m, and heat decomposition temperature is 265 DEG C.Observe under scanning electron microscope, as it is shown on figure 3,
Carbon dust arrangement densification, uniformly.
Claims (2)
1. an electroconductive printing ink is for the purposes of gas sensor electrode material, it is characterised in that described conduction off-set oil
Ink preparation method specifically comprises the following steps that
By modified urea-formaldehyde resin, carbon dust mixes with firming agent, simultaneously according to printing ink printing art requirement, adds reactive diluent and adjusts
Joint ink viscosity, can be prepared by the electroconductive printing ink for sensor electrode material, and wherein, the weight fraction of carbon dust is 3.5 ~
25 wt%, the weight fraction of firming agent is 5 wt%, and the weight fraction of reactive diluent is 15-20wt%, and remaining is modified urea-formaldehyde
Resin, its gross weight mark meets 100%；
Described modified urea-formaldehyde resin is that to use 1.5wt% polyvinyl alcohol and 4wt% tripolycyanamide be the Lauxite of modifier modification,
Specifically comprise the following steps that
(1) adding the polyvinyl alcohol of carbamide total amount 1.5% weight ratio, polyvinyl alcohol uses boiling water pre-activate, and uses 1% hydroxide
Sodium solution regulation pH=8 ~ 9, make the hydrogen bond formed between polyvinyl alcohol structures unit be destroyed, improve its reactivity；
(2) being joined in there-necked flask with first carbamide by formaldehyde and react, controlling aldehyde urea is 2 than F/U, uses 1% sodium hydroxide
PH value is regulated between 7 ~ 8 by solution, reacts 5 ~ 8 min, be subsequently added the preactivated PVA of step (1) gained, gradually at 45 DEG C
It is warming up to 75 DEG C of reaction 30 min；Then it is cooled to 70 DEG C, adds second batch carbamide and make F/U be 1.5, use 1% NaOH solution
Regulation system pH value is 5 ~ 6；After stopping heating continuation reaction 30 minutes, with 1% sodium hydroxide solution regulation pH value 7 ~ 8, add
The tripolycyanamide of the 3rd batch of carbamide and carbamide gross weight 4% makes F/U be 1.4, reacts 30 minutes, rapidly system is cooled to 40
Below DEG C, discharging, obtain modified urea-formaldehyde resin；
Described carbon dust is superconduction white carbon black, and particle diameter is 10 ~ 20nm, and resistivity is 0.8-1.0 Ω m, and content of ashes is less than
1.5%, do not allow containing semolina, remaining index meets GB/T3782-2006 standard；
Described reactive diluent is the Lauxite of low-solid content, and its solidification amount is less than 20%, and viscosity is less than 20 mpa.s；
The preparation method of the Lauxite of described low-solid content is three feeding methods, and with first carbamide, formaldehyde is added there-necked flask
In react so that F/U is 2, with 1% sodium hydroxide solution by pH value regulate between 7 ~ 8, at 45 DEG C react 5 ~ 8 min,
It is gradually heating to 75 DEG C of reaction 30 min subsequently；It is cooled to 70 DEG C, adds second batch carbamide and make F/U1.5, use 10% ammonium chloride
Solution regulation system pH value is 5 ~ 6, after stopping heating continuation reaction 30 minutes, with 1% sodium hydroxide solution regulation pH value 7 ~ 8,
Adding the 3rd batch of carbamide makes F/U be 1.4, reacts 30 minutes, rapidly system is cooled to less than 40 DEG C, and discharging obtains low solid
The Lauxite of content；
Described electrically conductive ink uses aeroge jet printing, and controlling to rotate viscosity is 10 ~ 3000mpa.s, or uses spray
Ink prints, and controlling to rotate viscosity is 10 ~ 80 mpa.s；
Gained solidification its resistivity of figure more than 250 DEG C, passes through scanning electron microscopic observation at 1 ~ 5 Ω m, heat decomposition temperature, it is seen that
Carbon powder particle after solidification presents the network structure of densification.
Electroconductive printing ink the most according to claim 1 is for the purposes of gas sensor electrode material, it is characterised in that
Described firming agent is one or more in aminoacid, organic dibasic acid or anhydride.
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| CN106953112B (en) * | 2017-05-09 | 2019-10-29 | 广东工业大学 | A kind of three-diemsnional electrode material preparation method and application |
| CN113310761B (en) * | 2021-05-08 | 2022-08-23 | 中国辐射防护研究院 | Preparation method of standard aerosol sample containing radionuclide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919940A (en) * | 2005-08-26 | 2007-02-28 | 上海复旦天臣研发中心有限公司 | Electron ink microcapsule and preparation method thereof |
| CN101719392A (en) * | 2009-12-30 | 2010-06-02 | 内蒙古大学 | Preparation method of screen printing water-based conductive paste based on carbon-copper composite packing |
| CN103319950A (en) * | 2013-06-19 | 2013-09-25 | 苏州凹凸彩印厂 | Carbon series electrically conductive ink |
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| EP2752470A1 (en) * | 2006-08-07 | 2014-07-09 | Inktec Co., Ltd. | Process for preparation of silver nanoparticles, and the compositions of silver ink containing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919940A (en) * | 2005-08-26 | 2007-02-28 | 上海复旦天臣研发中心有限公司 | Electron ink microcapsule and preparation method thereof |
| CN101719392A (en) * | 2009-12-30 | 2010-06-02 | 内蒙古大学 | Preparation method of screen printing water-based conductive paste based on carbon-copper composite packing |
| CN103319950A (en) * | 2013-06-19 | 2013-09-25 | 苏州凹凸彩印厂 | Carbon series electrically conductive ink |
Non-Patent Citations (1)
| Title |
|---|
| 环保型脲醛树脂胶粘剂的合成研究—三聚氰胺聚乙烯醇改性UF胶;曹晓玲等;《应用化学》;20080531;第37卷(第5期);第551-554,558页 * |
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